摘 要: 以4-甲基噻唑5-甲醛、异烟肼、苯甲酰肼、乙醇为原料合成了两种新型希夫碱：4-甲基噻唑5-甲醛缩异烟肼希夫碱（A）、4-甲基噻唑5-甲醛缩苯甲酰肼希夫碱（B），并通过红外光谱、核磁共振、质谱对其结构进行了表征，同时培养得到了它们的晶体，经X-射线衍射测定希夫碱A晶体属于单斜晶系，空间群为P21/n，晶胞参数分别为a = 8.623(2)Å，b = 10.477(3) Å, c = 13.016(4) Å, β = 97.879(7)°, V = 1164.8(6)Å3, Z = 2, μ(Mo Kα) = 0.266 mm-1, F(000) = 512, R1 = 0.0512, wR2 = 0.1221 [I>2σ(I)]；希夫碱B晶体也属于单斜晶系，空间群为P21/c，晶胞参数分别为a = 4.880(3)Å, b = 12.636(15)Å, c = 21.269(16) nm, β = 96.302(14)°, V = 1303.6(3)Å3, Z = 4, μ(Mo Kα) = 0.246 mm-1, F(000) = 552, R1 = 0.0475, wR2 = 0.1202 [I>2σ(I)]。71285

毕业论文关 键 词：噻唑，希夫碱、晶体结构、表征

Abstract: Two new Schiff bases, 4-methyl thiazole 5-formaldehyde condensation isoniazid Schiff base(A) and 4-methyl thiazole 5-formaldehyde condensation benzoyl hydrazine Schiff base(B) were synthesized with 4-methyl thiazole 5-formaldehyde, isoniazid, benzoyl hydrazine and ethanol. The structures of the two Schiff bases have been characterized by IR, NMR spectra, Mass spectrometry. And the crystal structures of A and B were obtained. According to X-ray single crystal diffraction, the A belongs to the monoclinic system, space group P21/n with cell parameters a=8.623(2) Å, b=10.477(3) Å, c =13.016(4)Å, β =97.879(7)°, V =1164.8(6)Å3, Z =4, μ(Mo Kα) =0.266 mm-1, F(000) =512, R1 = 0.0512, wR2 = 0.1221 [I>2σ(I)]. The B belongs to the monoclinic system, space group P21/c with cell parameters a=4.880(3)Å, b= 12.636(15)Å, c= 21.269(16) Å, β =96.302(14)°, V =1303.6(3)Å3, Z =4, μ(Mo Kα) =0.246 mm-1, F(000) =552, R1 =0.0475, wR2 =0.1202 [I>2σ(I)].

Keywords：Triazole, synthesis, crystal structure, characterization

目   录

1 前言 4

1.1 希夫碱及其配合物的主要合成方法 4

1.1.1直接合成法 4

1.1.2分步合成法 4

1.1.3返滴反应法 4

1.2 含噻唑环的希夫碱及其配合物的研究前景 5

2 实验部分 5

2.1 试剂 5

2.2 仪器 5

2.3 4-甲基噻唑5-甲醛缩异烟肼希夫碱（A）的合成 5

2.4 4-甲基噻唑5-甲醛缩苯甲酰肼希夫碱（B）的合成 6

2.5晶体的培养 6

3 结果与讨论 7

3.1 4-甲基噻唑5-甲醛缩异烟肼希夫碱（A）的表征 7

3.1.1 红外图谱及数据 7

3.1.2 核磁共振谱图及数据 8

3.1.3 质谱图及数据 9

3.2 4-甲基噻唑5-甲醛缩苯甲酰肼希夫碱（B）的表征 11

3.2.1 红外谱图及数据 11

3.2.2 核磁共振谱图及数据 12

3.2.3 质谱图及数据 13

3.3晶体结构的测定